Automatic shell freezing device



March 22, 1966 s. M. BROADWIN 3,241,250

AUTOMATIC SHELL FREEZING DEVICE Filed Jan. 5, 1965 2 Sheets-Sheet 1 INVENTQR. f/l/VUFL f2 BRU/IDW/A/ March 22, 1966 s. M. BROADWIN 3,241,250

AUTOMATIC SHELL FREEZING DEVICE Filed Jan. 5, 1965 2. Sheets-Sheet 2 llllllll ll 3.

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INVENTOR.

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AGENT United States Patent 3,241,250 AUTOMATIC SHELL FREEZING DEVICE Samuel M. Broadwin, New York, N.Y., assignor to Scientific Industries, Inc., Queens Village, N.Y., a corporation of New York Filed Jan. 5, 1965, Ser. No. 423,481 9 Claims. (Cl. 34-92) This invention relates to an apparatus for and a method of freeze drying liquids such as plasma and more particularly to the method of freeze drying of such liquids in the form of a shell within a container.

In the past the freeze drying of plasma within a container has been performed by rotating the container to thus spin the liquid into a shell-like form against the wall of the container to increase the freezing area. In this instance the container must be provided with a stopper or sealer.

It is an object of this invention to provide a device in which a plurality of containers for a liquid are retained in fixed relation with the device and in which the device is oscillated in a circular path Without rotating to spin the liquid within the container against the wall of the container in a shell-like form for freeze drying.

A further object of this invention is to provide a device in which a plurality of containers having a serni-spherical bottom are provided and are retained in a fixed relation with the device and in which the device is oscillated in a circular path Without rotating to spin the liquid by centrifugal force within the container into a shell formation against the wall of the container for freeze drying.

A still further object of this invention is to provide a device in which a plurality of spherical containers are provided and are retained in a fixed relation with the device and in which the device is oscillated in a circular path without rotating to spin the liquid by centrifugal force Within the container into a shell formation against the wall of the container for freeze drying.

It is a further object of this invention to provide a device in which a plurality of containers for a liquid are retained in a fixed relation with the device and a refrigerant means and a heating element are provided adjacent each container and in which the device is oscillated in a circular path without rotating to spin the liquid by centrifugal force within the container against the wall of the container in a shell-like form for freeze drying.

It is a further object of this invention to provide a device in which a plurality of containers for a liquid are retained in a fixed relation with the device and in which the device swings in a circular path on both a vertical and horizontal axis to provide a pitch and yaw without rotating to spin the liquid within the container by centrifugal force against the wall of the container in a shelllike form for freeze drying.

It is a further object of this invention to provide a device in which a plurality of containers for a liquid are retained in fixed relation with the device and in which the device is oscillated in a circular path without rotating to spin the liquid by centrifugal force within the container against the wall of the container in a shell-like form for shell freezing and in which the device is mounted within a vacuum chamber and means are provided to reduce the pressure in the chamber for the freeze drying process.

It is a still further object of this invention to provide a device in which a plurality of containers for a liquid are retained in a fixed relation with the device and in which the device swings in a circular path on both a vertical and horizontal axis to provide a pitch and yaw without rotating to spin the liquid by centrifugal force within the container against the wall of the container in a shell-like form for shell freezing and in which the device is mounted within a vacuum chamber and means are provided to reduce the pressure in the chamber for the freeze drying process.

Other objects of this invention shall be apparent by reference to the accompanying detailed description and the drawings in which FIG. 1 is a plan view of the automatic shell freezing device,

FIG. 2 is a cross sectional view taken on line 22 of FIG. 1,

FIG. 3 is a cross sectional view of a further embodi-' ment of the automatic shell freezing device, and

FIG. 4 illustrates the various forms of containers.

Referring to FIGS. 1 and 2 there is illustrated a shell freezing device 10. The device 10 is not necessarily round although it is illustrated circular in this embodiment. The device 10 comprises a solid body portion 11 having a plurality of circular bores 12 open to the upper surface 14 of body 11. Inserted into the bores 12 are container holding means which consist of a layer of foam material 15 and a conductive insert 16. The insert 16 may be circular in form as illustrated. Insert 16 is hollowed out to the configuration of the lower portion of the bottle to be mounted therein. In this instance the lower configuration is shown as semi-spherical. Thus a container 17 with a semi-spherical bottom is mounted in the insert 16 and retained or gripped by the foam layer 15 that extends above the insert 16. Insert 16 is also provided with a refrigerant coil 18. The refrigerant coil 18 is in turn.connected to the inlet and outlet of a refrigerant system to provide the necessary temperature reducing means for freeze drying. Insert 16 is also provided with a heater element 20. The heater element is in turn connected by wires 21-22 to a battery B, a switch S and a variable resistor control V so that the heater may be turned on by switch S and the degree of heat may be controlled by the variable resistor control V for purposes to be discussed later. The body 11 is supported upon a base 25 by a plurality of ball bearings or rollers 26. Base 25 also supports a motor 28. Motor 28 is connected to and drives gear 29. Gear 29 is meshed with a drive gear 30. Drive 30 is afiixed to a shaft 31 which extends into a bore 32 in body 11, bore 32 being open at the bottom face of body 11. Mounted on shaft 31 within bore 32 is a cam 33. It is to be noted that shaft 31 is positioned eccentric to the central axis of body 11. When the motor 28 is operated by a switch S1, the battery B1 will provide the power to operate motor 28. Thus motor 28 will drive through gear 29 through gear 30 to rotate shaft 31. Shaft 31 will in turn rotate cam 33. With cam 33 rotating since the rotation is eccentric to the central axis of bore 32, the body 11 will be moved in a vertical swinging oscillating movement. To prevent body 11 from rotating, body 11 is anchored against rotation by means of a plurality of springs 35 mounted in spaced relation about body 11. Springs 35 are attached to body 11 at 36 and are attached to a wall 37 at the opposite end. The wall 37 extends from base 25 and provides the vacuum chamber within which the device is mounted. The degree of oscillation is dependent upon the degree of eccentricity of shaft 31 and the size of cam 33 as indicated in dotted lines in FIG. 1. Both the degree of eccentricity and the size of cam 33 may be varied to provide the desired oscillating motion and the speed of the oscillating motion may be varied by providing the desired gear reduction between gears 29 and 30.

Referring to FIG. 3 there is illustrated a further embodiment of this invention in which a similar shell freeze drying device 10' is illustrated. In this embodiment the device is similarly constructed with a body portion 11 to u retain a plurality of containers 17 However in this embodiment body 11 must move in an oscillating motion in both a vertical and horizontal axis to provide a yaw and pitch for the containers mounted therein. The mechanism provided to produce this motion comprises a hollow base portion 40. The base portion extends to a central supporting housing 41 to support a central drive shaft 42 with a bearing 43. Mounted on the upper end of shaft 42 is a cam 44 whose cam face 45 abuts with the lower face of body 11. In the center of body 11 there is provided a semi-circular bore open to the bottom of body 11'. Shaft 42 is mounted eccentrically within bore 50 and cam 51 similar to cam 33 illustrated in FIGS. 1 and 2 is mounted on shaft 42 to bear against bore 50 so that as cam 51 rotates, it will in turn, as in FIGS. 1 and 2, produce an oscillating motion on a vertical axis to swing or oscillate body 11 in a circular motion without rotating body 11. Cam 44, being affixed to shaft 42, will rotate with shaft 42. Thus as cam 44 rotates, body 11 will oscillate on a vertical axis as illustrated in dotted lines. To prevent any rotation or attempt of body 11' to follow the rotation of the cams, there are a plurality of ties or springs 52 spaced about the periphery of body 11 attached at one end at 53 and spring 52 attached at its 0pposite end at 54 to base 40. Shaft 42 is connected to a gear 56. Gear 56 meshes with a drive gear 57, gear 57 being mounted on the motor shaft 58 of motor 59. Motor 59 is controlled by a switch 60 and switch 60 is in turn connected to a battery 61 and to motor 59. As in the previous embodiment, the gear ratio between gears 57 and 56 may be changed to provide the desired speed of rotation. The cams may also be changed to a different size to provide the desired degree of yaw and pitch. The complete device as illustrated in FIG. 3 is enclosed Within a vacuum chamber which includes a bottom wall 65 surrounding walls 66 and a removable top 67. The vacuum pump (not shown) is connected by means of a pipe 68 and valve 69 and inlet 70 to the vacuum chamber. This means is utilized for reduction of the pressure of the complete chamber. However in the event a single container 17 is mounted in body 11 there are provided auxiliary means comprised of valves 71, 72 and 73 providing separate inlets 74, 75 and 76. Utilizing any one of these inlets with a flexible hose 77, the hose 77 may be connected to a stopper 78. Stopper 78 may be of the type in which aspring pressed ball will close the container normally but will be lifted or released under vacuum. Thus with container 17 being oscillated on both a vertical and horizontal axis, the container may be evacuated by the vacuum means described to produce a freeze drying of the contents of container 17. Body 11' may also be provided with refrigerant means similar to that illustrated in FIGS. 1 and 2 and with heating elements similar to that illustrated in FIG. 2. However a further embodiment of cooling means is illustrated in FIG. 3. A condenser and refrigerant coil 80 is illustrated as mounted within the chamber of the freeze drying device 10 and a fan 81 is mounted behind the coil 80. Fan 81 is driven by a shaft 82 that may be connected to a motor (not shown). The condenser refrigerant coil 80 may also be connected by pipes 83 and 84 to refrigerant means (not shown). Thus the chamber Within the freezing device 10 may be cooled to thus produce the desired cooling around the containers 17. In this embodiment containers 17 are mounted in the oscillating body portion 11' and each container is retained by a wire or metal band 84 fitted to the periphery of the container 17. The wire or band 84 may also include a heater element 85, element 85 being connected by conductors 86-87 to an external control (not shown) to be utilized as already described in the previous embodiment.

Although we have described container 17 and illustrated container 17 in FIG. 2 with a semi-circular bottom, this type of container as illustrated in FIG. 4 may be preferable with a device as illustrated in FIGS. 1 and 2 to intil sure a perfect swirling of the liquid content to form an even frozen shell within container 17. However When we depart from this type of container to a flat bottom container 17 and either a round or square shape as illustrated in FIG. 4, the device illustrated in FIG. 3 will provide a better distribution of the contents to form the shell form within the container. And, when a container such as the globe shaped container 17" is provided, the device illustrated in FIG. 3 will increase the size of the shell form that will be produced within the container during shell freezing. It is to be understood that the insert 16 of FIG. 2 will be changed to receive the shape of container that is to be treated whether it be container 17, 17 or 17 The layer of foam 15 will simply be provided to grasp the container around the upper portion similar to the manner shown in FIG. 2.

In the method of shell freezing with the container 17 mounted as shown in FIG. 2, the liquid (plasma or serum) is generally mounted within the container before mounting it in the device It The refrigerant circuit is activated to provide the cooling effect upon insert 16 which in turn reacts on the walls of the container 17. The device is started in its oscillating motion thus producing a swirling of the liquid by centrifugal force within container 17 spreading out the liquid to a much greater wall area of container 17 and as the temperature reduces, the liquid forms or changes to a frozen formation on the wall of container 17 and will build up to the degree desired to form a shell-like form. The shell can then be treated for open freeze drying or may be treated in a closed chamber under vacuum for freeze drying. In a freeze drying process it is necessary to produce a vacuum in the chamber surrounding the device or to attach the vacuum system directly to the container 17 to thus remove the water vapor from the liquid (plasma) during the shell freezing process thus producing a dry shell freeze of the liquid (plasma).

Although we have described a shell freezing device for a plurality of containers to produce an oscillating motion either in a horizontal plane or in both a horizontal and vertical plane, the oscillating motion is to be produced without rotating the containers and although We have illustrated a form of device to produce this oscillating motion in the horizontal or in the vertical and horizontal plane, this invention shall not be limited by the particular cam means illustrated but shall include any means to produce this type of movement for the containers during a shell freezing process without departing from the spirit of this invention and this invention shall be limited only by the appended claims.

What is claimed is:

1. An apparatus for freeze drying liquids in a shell like form which includes a plurality of containers for retaining said liquid, said device having a chamber to retain a holder for said containers, said containers retained in a fixed relationship, a cooling coil and condenser within said chamber, a fan to circulate the air in said chamber for cooling, means for cooling said holder in an oscillating circular path in one plane without rotating to spin the liquid within each container, means to freeze said liquid in a shell like form Within each container.

2. In a device according to claim 1 in which means are provided to reduce the atmospheric pressure Within said chamber for vacuum freeze drying.

3. A device for treating of heat sensitive liquids which includes a centrifugal device for supporting a plurality of containers holding heat sensitive liquids to be treated, said centrifugal device supporting said containers in an upright fixed position, said centrifugal device having a central bore, a drive shaft, said drive shaft mounted ec centric to and within said central bore, a cam affixed to said drive shaft to bear against said centrifugal device to move said centrifugal device in an oscillating circular motion to produce the necessary centrifugal force for producing a swirling of the liquid into a shell like form in each container, said centrifugal device mounted within a chamber and resiliently retained to prevent rotation but allow oscillation, an evacuating means connected to said chamber to reduce the atmospheric pressure and produce a drying by evaporation affect on said liquid in said containers within said chamber, a valve to control the evacuating means and a valve to open said chamber to atmospheric pressure.

4. In a device according to claim 3 in which a refrigerant is circulated to produce cooling of said containers for freeze drying the heat sensitive liquid in said containers when in a shell like form.

5. A device for treating heat sensitive liquids which includes a centrifugal device for supporting a plurality of containers holding a heat sensitive liquid to be treated, said centrifugal device supporting said containers in an upright fixed position, said centrifugal device having a central bore and a flat bottom face, said central bore being eccentric to said centrifugal device, a drive shaft, said drive shaft mounted concentric to said centrifugal device and mounted within said central bore, an eccentn'c cam mounted on said drive shaft and within said central bore to bear against said centrifugal device to move said centrifugal device in an oscillating circular motion in a horizontal plane and a second cam mounted on said drive shaft below said centrifugal device to bear against said flat bottom face to rock said centrifugal device in a vertical plane to produce the necessary centrifugal force and swirling motion of the liquid within said containers for shell freezing of the liquid in each container, said centrifugal device mounted within a chamber and resiliently retained to prevent rotation but allow oscillation and rocking, an evacuating means connected to said chamber to reduce the atmospheric pressure and produce a drying by evaporation on said liquid in said containers within said chamber, a valve to control the evacuating means and a valve to open said chamber to atmospheric pressure.

6. In a device according to claim 5 in which cool air is circulated to cool said containers for freezing the heat sensitive liquid while in a shell like form.

7. In a device according to claim 5 in which a heater and control are included in said device to permit controlling the temperature during the shell freezing.

8. A device for treating of heat senstive liquids which includes a centrifugal device for supporting a plurality of containers holding heat sensitive liquids to be treated, said centrifugal device supporting said containers in an upright fixed position, said centrifugal device having a central bore, a drive shaft, said drive shaft mounted eccentric to and within said central bore, a cam aflixed to said drive shaft to bear against said centrifugal device to move said centrifugal device in an oscillating circular motion to produce the necessary centrifugal force for producing a swirling of the liquid into a shell like form in each container, said centrifugal device mounted within a chamber and resiliently retained to prevent rotation but allow oscillation, an evacuating means connected to each container to reduce the atmospheric pressure and produce a drying by evaporation of said liquid in said container, a valve to control the evacuating means and a valve to open said container to atmospheric pressure.

9. A device for treating heat sensitive liquids which includes a centrifugal device for supporting a plurality of containers holding a heat sensitive liquid to be treated, said centrifugal device supporting said containers in an upright fixed position, said centrifugal device having a central bore and a fiat bottom face, said central bore being eccentric to said centrifugal device, a drive shaft, said drive shaft, mounted concentric to said centrifugal device and mounted within said central bore, an eccentric carn mounted on said drive shaft and within said central bore to bear against said centrifugal device to move said centrifugal device in an oscillating circular motion in a horizontal plane and a second cam mounted on said drive shaft below said centrifugal device to bear against said flat bottom face to rock said centrifugal device in a vertical plane to produce the necessary centrifugal force and swirling motion of the liquid within said containers for shell freezing of the liquid in each container, said centrifugal device mounted within a chamber and resiliently retained to prevent rotation but allow oscillation and rocking, an evacuating means connected to each container to reduce the atmospheric pressure and produce a drying by evaporation of said liquid in said container, a valve to control the evacuating means and a valve to open said container to atmospheric pressure.

References Cited by the Examiner UNITED STATES PATENTS 1,275,547 8/1918 Forrest 34-92 2,247,978 7/ 1941 Van Arkel 259-72 2,373,806 4/1945 Barnes 34-5 2,655,007 10/1953 Lozar 62-381 2,829,528 4/1958 Hulick 74-86 2,859,534 11/1958 Copson 34-92 2,907,117 10/1959 Parkinson 34-92 3,159,384 12/1964 Davis 259-72 3,199,216 8/ 1965 Broadwin 34-92 3,203,108 8/1965 Broadwin 34-92 WILLIAM J. WYE, Primary Examiner. 

1. AN APPARATUS FOR FREEZE DRYING LIQUIDS IN A SHELL LIKE FORM WHICH INCLUDES A PLURALITY OF CONTAINERS FOR RETAINING SAID LIQUID, SAID DEVICE HAVING A CHAMBER TO RETAIN A HOLDER FOR SAID CONTAINERS, SAID CONTAINERS RETAINED IN A FIXED RELATIONSHIP, A COOLING COIL AND CONDENSER WITHIN SAID CHAMBER, A FAN TO CIRCULAR THE AIR IN SAID CHAMBER FOR COOLING, MEANS FOR COOLING SAID HOLDER IN AN OSCILLATING CIRCULAR PATH IN ONE PLANE WITHOUT ROTATING TO SPIN THE LIQUID WITHIN EACH CONTAINER, MEANS TO FREEZE SAID LIQUID IN A SHELL LIKE FORM WITHIN EACH CONTAINER. 